High-specific surface silkworm excrement-porous carbon-MOFs composite material prepared through impregnation method and preparation method and application thereof

A high specific surface, composite material technology, applied in the field of carbon materials, can solve the problems of non-target biological damage to the environment, excessive pesticide residues in agricultural products, low pesticide utilization efficiency, etc., to achieve the effect of easy control, convenient operation and high adsorption capacity

Active Publication Date: 2017-02-01
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, only a small amount of pesticides can reach the crop target site in a specific time, and most of the pesticides are directly released into the natural environment, resulting in low pesticide util

Method used

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  • High-specific surface silkworm excrement-porous carbon-MOFs composite material prepared through impregnation method and preparation method and application thereof
  • High-specific surface silkworm excrement-porous carbon-MOFs composite material prepared through impregnation method and preparation method and application thereof
  • High-specific surface silkworm excrement-porous carbon-MOFs composite material prepared through impregnation method and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A preparation method of silkworm excrement porous carbon MOFs composite material with high specific surface impregnation method, comprising the following steps,

[0039](1) Mix and swell the original silkworm excrement and deionized water according to the mass-to-body ratio of 1:100. After swelling at 30°C for 3.0 hours, remove the silkworm excrement and freeze-dry it. First, freeze and pretreat at -20°C for 4 hours. Then lower the temperature to -60° C. and freeze-dry for 24 hours to obtain freeze-dried silkworm excrement.

[0040] (2) freeze-dried silkworm excrement in N 2 In the atmosphere, the temperature was raised to 300°C at a rate of 5°C / min, and kept at 300°C for 5.0h to carry out the pore expansion reaction. After naturally cooling down to room temperature, the obtained solid was dissolved in 1mol / L HCl to clean the material, and then Wash with deionized water to pH ≈ 7, then centrifuge, place in an oven to dry overnight, and obtain the silkworm excrement-bas...

Embodiment 2

[0045] (1) Mix and swell the original silkworm excrement and deionized water according to the mass-to-body ratio of 1:120. After swelling at 35°C for 2.5 hours, remove the silkworm excrement and freeze-dry it. First, freeze it at -20°C for 3 hours. Then lower the temperature to -55° C. and freeze-dry for 36 hours to obtain freeze-dried silkworm excrement.

[0046] (2) Raise the freeze-dried silkworm excrement to 350°C at a heating rate of 5°C / min in an Ar atmosphere, and keep it at 350°C for 4.0h to carry out the pore expansion reaction. After naturally cooling down to room temperature, dissolve the obtained solid Wash the material in 1mol / L HCl, then use deionized water to wash to pH ≈ 7, then centrifuge, place in an oven to dry overnight, and obtain silkworm excrement-based hierarchical porous carbon material after drying.

[0047] (3) Combine the silkworm excrement-based hierarchical porous carbon material with 1.0mol / L Fe 2 (NO 3 ) 3 The solution was shaken and mixed ac...

Embodiment 3

[0051] (1) Mix and swell the original silkworm excrement and deionized water according to the plastid ratio of 1:140, swell at 40°C for 2.0 hours, remove the silkworm excrement and freeze-dry it, and first freeze and pretreat it at -25°C for 2 hours, Then lower the temperature to -50° C. and freeze-dry for 48 hours to obtain freeze-dried silkworm excrement.

[0052] (2) freeze-dried silkworm excrement in N 2 In the atmosphere, the temperature was raised to 400°C at a rate of 5°C / min, and kept at 400°C for 3.0h to carry out the pore expansion reaction. After cooling down to room temperature naturally, the obtained solid was dissolved in 1mol / L HCl to clean the material, and then Wash with deionized water to pH ≈ 7, then centrifuge, place in an oven to dry overnight, and obtain the silkworm excrement-based hierarchical porous carbon material after drying.

[0053] (3) Combine the silkworm excrement-based hierarchical porous carbon material with 1.5mol / L Cu(NO 3 ) 2 The soluti...

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Abstract

The invention discloses a high-specific surface silkworm excrement-porous carbon-MOFs composite material prepared through an impregnation method and a preparation method and application thereof. The preparation method comprises the steps that firstly, silkworm excrement and water are subjected to mixing swelling and then freeze-dried; secondly, the freeze-dried silkworm excrement is subjected to a carbonization chambering reaction in protection gas, and then cleaning, centrifuging and drying are conducted to obtain a silkworm excrement-based porous carbon material; thirdly, a metal salt solution and the material are stirred, mixed, centrifuged and dried, and high-dispersion metal oxides are formed on the surface of the silkworm excrement-based porous carbon material by introducing oxygen under the plasma modification conditions; fourthly, MOFs grow on the surface of the silkworm excrement-based carbon material by taking the high-dispersion metal oxides as precursors through a microwave radiation method; lastly, suction filtration and drying are conducted, and the high-specific surface silkworm excrement-porous carbon-MOFs composite material prepared through the impregnation method is obtained. The material can be applied to sustained or controlled release of pesticides. The composite carbon material obtained through the method has the high specific surface and carboxy groups and can achieve the high adsorption capacity and the good sustained or controlled release effect on the pesticides.

Description

technical field [0001] The invention belongs to the technical field of carbon materials, and in particular relates to a high specific surface impregnation silkworm excrement porous carbon MOFs composite material and a preparation method and application thereof. Background technique [0002] Pesticides can effectively control the harm of diseases, insects, weeds and other harmful organisms to crops. As an important means of chemical control, pesticides play an irreplaceable role in agricultural production. However, only a small amount of pesticides can reach the crop target site in a specific time, and most of the pesticides are directly released into the natural environment, resulting in low pesticide utilization efficiency. These ineffective pesticides will cause many negative problems such as excessive pesticide residues in agricultural products, damage to non-target organisms, and environmental pollution. How to effectively improve the utilization efficiency and targeted...

Claims

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Application Information

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IPC IPC(8): B01J20/24B01J20/28B01J20/32A01G13/00
CPCA01G13/00B01J20/0218B01J20/0225B01J20/0237B01J20/24B01J20/28066B01J20/28095B01J20/3206
Inventor 赵祯霞周凯彬胡鹏赵钟兴
Owner GUANGXI UNIV
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